Crystal Structure Studies on p-Substitutedbenzenesulphonamides 4-X-C6H4SO2NH2 (X = CH3, NH2 F, Cl or Br)

2003 ◽  
Vol 58 (11) ◽  
pp. 656-660 ◽  
Author(s):  
B. Thimme Gowda ◽  
K. Jyothi ◽  
Jozef Kožíšek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structures ◽  
Phenyl Ring ◽  
Bond Angle ◽  
Amine Group ◽  
Torsion Angles ◽  
Bond Angles ◽  
Lattice Constants ◽  
Bond Lengths ◽  
Crystal Type ◽  
Uniform Substitution

Effect of ring substitution on the crystal structures of p-substitutedbenzenesulphonamides, p-XC6H4SO2NH2 (X = F, Cl, Br, CH3 or NH2) has been studied by determining the crystal structures of 4-chlorobenzenesulphonamide (4-ClC6H4SO2NH2) and 4-bromobenzenesulphonamide (4-BrC6H4SO2NH2) and analyzing the results along with the structures of 4-methylbenzenesulphonamide (4-CH3C6H4SO2NH2), 4-fluorobenzene-sulphonamide (4-FC6H4SO2NH2) and 4-aminobenzenesulphonamide (4-NH2C6H4SO2NH2). The crystal type, space group, formula units and lattice constants in Å of new structures are: (4-ClC6H4SO2NH2); monoclinic, P21/n, Z = 4, a = 6.6276(10), b = 16.219(3), c = 7.5716(10), β = 93.387(14)°; (4-BrC6H4SO2NH2): monoclinic, P 21/n, Z = 4, a = 6.5660(10), b = 16.4630(10), c = 7.6900(10), β = 92.760(10)°. Orientation of the amine group with respect to the phenyl ring is given by the torsion angles C(2)-C(1)-S-N: 70.9° and C(6)-C(1)-S-N: −108.5°. Similarly, the orientation of S, O(1) and O(2) with respect to the ring are given by torsion angles. The comparison of bond lengths and bond angles of 4-fluoro-, 4-chloro-, 4-bromo-, 4-methyl- and 4-amino-benzenesulphonamides reveal that the S-N and C-S bond lengths decrease with the introduction of electron-withdrawing substituents such as F, Cl or Br, while these groups do not have significant effects on the S-O distances. The effect on ring C-C distances was not uniform. Substitution of F, Cl or Br decreases the O-S-N bond angle, but increases the O-S-N, N-S-C(1) and C(3)-C(4)-C(5) bond angles.

Effect of Substituent on Crystal Structures of N-(Substituted- phenyl)-2,2,2-Trichloroacetamides, 2/3/4-XC 6 H 4 .NHCO.CCl 3 (X = Cl, NO 2 or CH 3 )

2000 ◽  
Vol 55 (8) ◽  
pp. 711-720 ◽  
Author(s):  
B. Thimme Gowda ◽  
Helmut Paulus ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structures ◽  
Phenyl Ring ◽  
Room Temperature ◽  
Ortho Position ◽  
Asymmetric Unit ◽  
Strong Electron ◽  
Bond Angles ◽  
Lattice Constants ◽  
Crystal Type

Abstract The crystal structures of N-(substitutedphenyl)-2,2,2-trichloroacetamides of the type 2/3/4-XC6H4.NHCO.CCl3 (X = CI, NO2 or CH3), namely, N-(3-nitrophenyl)-2,2,2-trichloroacetamide,3-NO2C6H4.NHCO.CCl3 (m-NO2PhTCA); N-(4-nitrophenyl)-2,2,2-trichloroacetamide,4-NO2C6H4.NHCO.CCl3 (p-NO2PhTCA); N-(2-chlorophenyl)-2,2,2-trichloroacetamide,2-ClC6H4.NHCO.CCl3 (o-ClPhTCA) and N-(4-chlorophenyl)-2,2,2-trichloroacetamide, 4-C1C6H4.NHCO.CCl3 (p-ClPhTCA) have been determined at room temperature. The presentdata are analysed along with our earlier crystal structures of N-(2-nitrophenyl)-2,2,2-trichloroacetamide,2-NO2C6H4.NHCO.CCl3 (o-NO2PhTCA); N-(4-methylphenyl)-2,2,2-trichloroacetamide,4-CH3C6H4. NHCO.CCl3 (p-CH3PhTCA); N-(phenyl)-2,2,2-trichloroacetamide,C6H5.NHCO.CCl3 (PhTCA); N-chloro-N-(phenyl)-2,2,2-trichloroacetamide, C6H5.NClCO.CCl3(NClPhTCA); and finally with N-(phenyl) acetamide, C6H5.NHCO.CH3 (PhA). The crystal type,space group, formula units and lattice constants in Å of the new structures are; m-NO2PhTCA:triclinic, PI, Z = 4, a = 7.493(3), b = 9.992(3), c = 15.225(5), α = 84.16(2)°, β = 82.59(2)°, γ =84.92(2); p-N02PhTCA: monoclinic, P21/n, Z = 4, a = 5.807(2), b = 15.354(6), c = 12.475(5),β = 92.28(2)°; o-ClPhTCA: orthorhombic, Pna21, Z = 4, a = 8.769(2), b = 12.838(3), c = 9.578(2)and p-ClPhTCA: orthorhombic, Pbca, Z = 8, a = 9.742(4), b = 10.031(4), c = 23.110(9). Thecompounds, m-NO2PhTCA, o-NO2PhTCA and p-CH3PhTCA show two molecules each in theirasymmetric units. This is in agreement with the multiple lines observed in the 35Cl NQR spectraof the latter two compounds. But the presence of two molecules in the asymmetric unit of m-NO2PhTCA indicates that it may undergoe a phase transition below room temperature. The bondlengths and bond angles are normal except for some deviations. The presence of strong electronwithdrawing group at the ortho position of the phenyl ring and N-chlorination of the amide willhave significant effect on some bond distances and bond angles.

Structural Studies on Substituted N-(phenyl)-2,2-DichIoroacetamides, 2/4-XC6H4 NHCO CHCI2 (X = H, Cl or CH3)

2001 ◽  
Vol 56 (5) ◽  
pp. 386-394 ◽  
Author(s):  
B. Thimme Gowda ◽  
Helmut Paulus ◽  
Hartmut Fuess
Keyword(s):  
Bond Length ◽  
Crystal Structures ◽  
Phenyl Ring ◽  
Side Chain ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
Lattice Constants ◽  
Crystal Type ◽  
Electron Withdrawing Group

Abstract The effect of substitution in the phenyl ring on the crystal systems of amides of the type, 2/4-XC6H4-NHCO-CHCl2 (X = H, Cl or CH3), has been studied by determining the crystal structures of the compounds, iV-(phenyl)-2,2-dichloroacetamide, C6H5-NHCO-CHCl2 (PhDCA); N-(2-chlorophenyl)-2,2-dichloroacetamide, 2-ClC6H4-NHCO-CHCl2 (o-ClPhDCA), jY-(4-chlorophenyl)-2,2-dichloroacetamide, 4-ClC6H4-NHCO-CHCl2 (p-ClPhDCA) and N -(4-methylphenyl)-2,2-dichloroacetamide, 4-CH3C6H4-NHCO-CHCl2 (p-CH3PhDCA) and analysed the data along with our earlier crystal structures of the compounds, N-(phenyl)-2,2,2-trichloro-acetamide (PhTCA), N-(2-chlorophenyl)-2,2,2-trichloroacetamide (o-ClPhTCA), N -(4-chloro-phenyl)-2,2,2-trichloroacetamide (p-ClPhTCA), N-(4-methylphenyl)-2,2,2-trichloroacetamide (p-CH3PhTCA); N-chloro-N-(phenyl)-2,2-dichloroacetamide (NClPhDCA), N-chloro-N-(phenyl)-2,2,2-trichloroacetamide (NClPhTCA) and N-(phenyl) acetamide (PhA). The crystal type, space group, formula units and lattice constants in A of the new structures are; PhDCA: monoclinic, P 21/c, Z = 4, a = 8.785(3), b = 11.139(4), c = 9.521(3), ß = 97.47(2)°; o-CIPhDCA: monoclinic, P 21/c, Z = 4, a = 4.711(2), b = 11.234(6), c = 19.191(8), ß = 98.12(2)°; p-CIPhDCA: monoclinic, P 21/c, Z = 8, a = 18.627(5), b = 11.533(3), c = 9.583(3), ß = 102.43(2)°, and /?-CH3PhDCA: orthorhombic, Pbca, Z = 8, a = 9.464(3), b = 9.894(3), c = 21.973(7). The compound p-ClPhDCA shows two molecules in its asymmetric unit. This is in agreement with the multiple lines observed in the 35Cl NQR spectra of the compound. The crystal systems of the chlorosubstituted and methyl substituted chloroacetamides get interchanged on replacement of the side chain -CHCl2 by -CCl3. C(i)-C(j) ring distances show no significant variations with the substitution either at the side chain or in the phenyl ring. C(ring)-N and C (0)-N bond distances are also not much affected by either ring or side chain substitution, but are affected by N-chlorination, while the C -0 bond length is slightly shortened by the replacement of the -CH3 group by -CCl3, the introduction of electron withdrawing group into the phenyl ring or by N-chlorination. Deviations of C2(ring)-Cl(ring)-N, C6(ring)-Cl(ring)-N and C (ring)-N-C(0) bond angles from 120° narrow down on substitution either in the phenyl ring or in the side chain, but the latter increases on W-chlorination of the compounds.

Die Kristallstrukturen der silylierten Phosphanimine Me3SiNPPh3 und Me3SiNPPh2 - C2H4 - PPh2NSiMe3 / Crystal Structures of the Silylated Phosphanimines Me3SiNPPh3 und Me3SiNPPh2 - C2H4 - PPh2NSiMe3

1995 ◽  
Vol 50 (7) ◽  
pp. 1050-1054 ◽  
Author(s):  
Frank Weller ◽  
Hak-Chul Kang ◽  
Werner Massa ◽  
Thilo Rübenstahl ◽  
Frank Kunkel ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Bond Angle ◽  
Structure Refinement ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Single Bonds

The crystal structures of two silylated phosphanimines have been determined. Me3SiNPPh3: Space group P 1̃, Z = 2, structure refinement with 2907 observed unique reflections with Fo > 5 σ(Fo), R = 0.052. Lattice dimensions at 19 °C: a = 876.6(1), b = 1125.8(1), c = 1151.2(1) pm, α = 61.71(1)°, β = 88.08(1)°, γ = 87.18(1)°. The compound forms monomeric molecules with a SiNP bond angle of 140.2° and bond lengths PN of 154.2 pm and SiN of 168.6 pm which correspond with PN double and SiN single bonds. Me3SiNPPh2 - C2H4 -PPh2N SiMe3: Space group P31, Z = 3, structure refinement with 4251 independent reflections, R = 0.061 for 3587 reflections with I > 2σ(I). Lattice dimensions at - 80 °C: a = b = 1591.4(1), c = 1165.8(1) pm. The compound forms monomeric molecules with a c/s-conformation of the PNSiMe3 groups. Bond angles and bond lengths (average) are SiNP = 140.8°, PN = 153.8 pm, SiN = 165.6 pm.

35CI NQR and Structural Studies of N-(2,6-Dichlorophenyl)-Amides, 2,6-Cl2C6H3-NHCO-R (R = H or CH3-y Xy and X = CH3 or CI; y = 0,1, 2 or 3)

2000 ◽  
Vol 55 (9-10) ◽  
pp. 791-800 ◽  
Author(s):  
B. Thimme Gowda ◽  
Helmut Paulus ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Crystal Symmetry ◽  
Side Chain ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
Space Group ◽  
Lattice Constants ◽  
Bond Lengths ◽  
Crystal Type

The effect of side chain substitution on the 35CI NQR and crystal structure of amides of the type N-(2,6-dichlorophenyl)-amides, 2,6-Cl2C6H3-NHCO-R (R = H or CH3_yXy where X = CH3 or CI and y = 0, 1, 2 or 3), has been studied by measuring the 35C1 NQR spectra and determining the crystal structures of the compounds N-(2,6-dichlorophenyl)-formamide, 2,6-Cl2C6H3- NHCO-H (DCPFA); N-(2,6-dichlorophenyl)-2-methylacetamide(propionamide), 2,6-Cl2C6H3- NHCO-CH2CH3 (DCPMA); N-(2,6-dichlorophenyl)-2,2-dimethylacetamide(isobutyramide), 2,6- Cl2C6H3-NHCO-CH(CH3 ) 2 (DCPDMA) and N-(2,6-dichlorophenyl)-2,2,2-trimethylacetamide (neopentylamide), 2,6-Cl2C6H3-NHCO-C(CH3)3 (DCPTMA), and by analysing the present data along with the 35CI NQR spectra and / or crystal structures of the compounds, 2,6-dichloroaniline, 2,6-Cl2C6H3-NH2 (DCA), N-(2,6-dichlorophenyl)-acetamide, 2,6-Cl2C6H3--NHCO-CH3 (DCPA), N-(2,6-dichlorophenyl)-2-chloroacetamide, 2,6-Cl2C6H3-NHCO-CH2Cl (DCPCA), N- (2,6-dichlorophenyl)-2,2-dichloroacetamide, 2,6-Cl2C6H3-NHCO-CHCl2 (DCPDCA) and N- (2,6-dichlorophenyl)-2,2,2-trichloroacetamide, 2,6-Cl2C6H3-NHCO-CCl3 (DCPTCA). The crystal type, space group, formula units and lattice constants in A of the new structures are;DCPFA: orthorhombic, Pbca, Z = 8, a = 8.593(3), b = 12.728(4), c = 14.376(4); DCPMA: orthorhombic, P212121, Z = 4, a = 4.774(2), b = 10.961(5), c = 19.562(8); DCPDMA: monoclinic, P21/c, Z = 4, a = 9.901(4), b = 13.785(5), c = 9.060(3), ß = 103.58(2)° and DCPTMA: monoclinic, P21/n, Z = 8, a = 16.047(5), b = 9.882(3), c = 16.270(5) ß = 102.12(1)°. The compound, DCPTMA shows two molecules in its asymmetric unit. This is in agreement with the multiple lines observed in the 35CI NQR spectra of the compound. The conversion of DCA (monoclinic) into it's various acid amides DCPFA, DCPA, DCPMA, DCPDMA, DCPTMA, DCPCA and DCPTCA affects it's crystal symmetry. The replacement of the side chain CH3 in DCPA by the H atom or substitution of either a CH3 group or a CI atom for one of the H atoms in the side chain CH3 or replacement of the two ring CI atoms by the H atoms changes it's crystal symmetry from monoclinic to orthorhombic, while the substitution of 2 or all the 3 H atoms in the CH3 group of DCPA by 2 or 3 CH3 groups or CI atoms restores it's crystal symmetry back to the monoclinic type. The bond lengths and bond angles are normal except for some deviations.

Synthesis and Crystal Structures of Three Carboxylate- Bridged Tetranuclear Copper(II) - Lanthanide(III) Complexes of Ph3P+CH2CH2CO2−

1999 ◽  
Vol 52 (10) ◽  
pp. 983 ◽  
Author(s):  
Yang-Yi Yang ◽  
Seik Weng Ng ◽  
Xiao-Ming Chen
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Metal Atoms ◽  
Apical Site

Three tetranuclear copper(II)–lanthanide(III) complexes of triphenylphosphoniopropionate (Ph3P+CH2CH2CO2−,tppp), namely [Cu2Ln2(tppp)8(H2O)8](ClO4)10·2H 2 O [Ln = EuIII, NdIII or CeIII], were synthesized and characterized by crystallography. The EuIII complex crystallizes in the triclinic space group P1 – with a 16.249(7), b 17.185(11), c 17.807(11) Å, α 69.750(10), β 89.230(10), γ 84.070(10)˚, V 4639(5) Å3, Z 1. In the crystal structures, four tppp ligands bridge a pair of CuII and tetraaquo-EuIII atoms (Cu···Eu 3.527(2) Å) through their µ2-carboxylato ends to form a dinuclear subunit; two of these subunits are additionally linked by one of the CuII -bonded carboxylato oxygen ends, across a centre of inversion, to furnish a dimeric tetranuclear [Cu(tppp)4 Eu(H2O)4]2 species (Cu···Cu 3.323(2) Å). This CuII -bonded oxygen atom occupies the apical site of the square-pyramidal coordination environment of the CuII atom. The EuIII atom is eight-coordinated in a square-antiprismatic geometry. The NdIII and CeIII complexes are isomorphous to the EuIII complex, and only minor differences in bond lengths and bond angles involving the metal atoms are noted.

Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu and Ni coordination compounds

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
Tarlok Singh Lobana ◽  
Mani Kaushal ◽  
Robin Bhatia ◽  
Ritu Bala ◽  
Ray J. Butcher ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Coordination Compounds ◽  
Bond Angle ◽  
Donor Atom ◽  
Neutral Form ◽  
Bond Angles ◽  
Square Planar ◽  
Tetrahedral Bond

In this investigation, the crystal structures of the thio-ligands 3-formylpyridine 4-phenylthiosemicarbazone (C13H12N4S, 1) and 4-benzoylpyridine 4-ethylthiosemicarbazone (C15H16N4S, 2), and of two new coordination compounds, chlorido(3-formylpyridine 4-phenylthiosemicarbazone-κS)bis(triphenylphosphane-κP)copper(I) acetonitrile monosolvate, [CuCl(C13H12N4S)(C18H15P)2]·CH3CN, 3, and bis(3-formylpyridine 4-ethylthiosemicarbazonato-κ2 N 1,S)nickel(II), [Ni(C9H11N4S)2], 4, are reported. In complex 3, the thio-ligand coordinates in a neutral form to the Cu atom through its S-donor atom, and in complex 4, the anionic thio-ligand chelates to the Ni atom through N- and S-donor atoms. The geometry of complex 3 is distorted tetrahedral [bond angles 99.70 (5)–123.23 (5)°], with the P—Cu—P bond angle being the largest, while that of complex 4 is square planar, with trans-S—Ni—S and N—Ni—N bond angles of 180°.

(2-Methyldithiobenzoato-κS)(triphenylphosphine-κO)gold(I)

2006 ◽  
Vol 62 (4) ◽  
pp. m889-m890 ◽  
Author(s):  
Jennifer S. Macalindong ◽  
Frank R. Fronczek ◽  
Judith A. Schuerman ◽  
Joel Selbin ◽  
Steven F. Watkins
Keyword(s):  
Title Compound ◽  
Asymmetric Unit ◽  
Gold Complexes ◽  
Torsion Angles ◽  
Bond Angles ◽  
Bond Lengths

The asymmetric unit of the title compound, o-CH3(C6H4)C(S)S–Au–P(C6H5)3 or [Au(C8H7S2)(C18H15P)], consists of two quasi-linear gold complexes. The S—Au—P bond angles [173.83 (2), 175.03 (2)°], S—Au bond lengths [2.3240 (6), 2.3329 (6) Å] and Au—P bond lengths [2.2568 (6), 2.2632 (6) Å] are consistent with previously reported values. The major difference in the two molecules is that the o-methylphenyl rings are twisted with respect to the dithiocarboxyl planes by 73.0 (3)° and 46.6 (3)°, as measured by S—C—C—C torsion angles.

scholarly journals Bis(flavonolato-κ2O,O′)dioxidoosmium(VI) dichloromethane disolvate

IUCrData ◽  
2017 ◽  
Vol 2 (9) ◽  
Author(s):  
Will Lynch ◽  
Clifford Padgett
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Metal Cation ◽  
Bond Angle ◽  
Central Metal ◽  
Bond Angles ◽  
Bond Lengths ◽  
Solvent Molecules

In the crystal structure of the title solvatedtrans-dioxidoosmium(VI) flavonolate (flav) complex, [Os(C15H9O3)2O2]·2CH2Cl2or [Os(flav)2O2]·2CH2Cl2, the two dichloromethane solvent molecules have nonclassical hydrogen-bonding contacts at or greater than 3.18 Å. The pseudo-octahedrally coordinated central metal cation is observed with all donor atoms being oxygen. The Os=O bond lengths are 1.721 (5) and 1.728 (5) Å, with a 170.4 (2)° bond angle. The O—Os bond lengths arising from the flanvonolate ligand are observed to all be slightly over 2.0 Å. The chelate bond angles arising from the flavonolate O atoms with the osmium cation are constrained by the ligand at 80.72 (18) and 80.92 (17)°.

O-Benzoyl side-chain conformations in 2,3,4,6-tetra-O-benzoyl-β-D-galactopyranosyl-(1→4)-1,2,6-tri-O-benzoyl-β-D-glucopyranose (ethyl acetate solvate) and 1,2,4,6-tetra-O-benzoyl-β-D-glucopyranose (acetone solvate)

2019 ◽  
Vol 75 (2) ◽  
pp. 161-167 ◽  
Author(s):  
Toby Turney ◽  
Qingfeng Pan ◽  
Wenhui Zhang ◽  
Allen G. Oliver ◽  
Anthony S. Serianni
Keyword(s):  
Ethyl Acetate ◽  
Bond Angle ◽  
Solution Nmr ◽  
Side Chain ◽  
Nmr Studies ◽  
Torsion Angles ◽  
Bond Lengths ◽  
Side Chain Conformation ◽  
Chain Conformations ◽  
Good Agreement

The crystal structures of 2,3,4,6-tetra-O-benzoyl-β-D-galactopyranosyl-(1→4)-1,2,6-tri-O-benzoyl-β-D-glucopyranose ethyl acetate hemisolvate, C61H50O18·0.5C4H8O2, and 1,2,4,6-tetra-O-benzoyl-β-D-glucopyranose acetone monosolvate, C34H28O10·C3H6O, were determined and compared to those of methyl β-D-galactopyranosyl-(1→4)-β-D-glucopyranoside (methyl β-lactoside) and methyl β-D-glucopyranoside hemihydrate, C7H14O6·0.5H2O, to evaluate the effects of O-benzoylation on bond lengths, bond angles and torsion angles. In general, O-benzoylation exerts little effect on exo- and endocyclic C—C and endocyclic C—O bond lengths, but exocyclic C—O bonds involved in O-benzoylation are lengthened by 0.02–0.04 Å depending on the site of substitution. The conformation of the O-benzoyl side-chains is highly conserved, with the carbonyl O atom either eclipsing the H atom attached to a 2°-alcoholic C atom or bisecting the H—C—H bond angle of an 1°-alcoholic C atom. Of the three bonds that determine the side-chain geometry, the C—O bond involving the alcoholic C atom exhibits greater rotational variability than the remaining C—O and C—C bonds involving the carbonyl C atom. These findings are in good agreement with recent solution NMR studies of the O-acetyl side-chain conformation in saccharides.

Kupfer(I)-chlorid-Addukte von Phosphoraniminen Die Kristallstrukturen von Ph 3 PNPh * CuCl und von 2,3-Bis(triphenylphosphoranylidenamino)maIeinsäure-N-methylimid- Kupfer(I)-chlorid / Copper(I) Chloride Adducts of Phosphoranimines The Crystal Structures of Ph3 PNPh·CuCl and of 2,3-Bis(triphenylphosphoranylideneamino)maleic Acid N-Methylimide Copper(I) Chloride

1988 ◽  
Vol 43 (1) ◽  
pp. 5-11 ◽  
Author(s):  
Andrea Maurer ◽  
Dieter Fenske ◽  
Johannes Beck ◽  
Joachim Strähle ◽  
Eberhard Böhm ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Maleic Acid ◽  
Bond Angle ◽  
Asymmetric Unit ◽  
Space Group ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Independent Molecules

Abstract The title compounds Ph3PNPh · CuCl (1) and (Ph3P)2 N2 C4O2 (NMe) CuCl (2) have been prepared by the reactions of CuCl with the corresponding phosphoranimines Ph3PNPh and 2.3-bis(triphenylphosphoranylideneamino)maleic acid N-methylimide, respectively. Both com-plexes were characterized by their IR spectra as well as by crystal structure determinations. Ph3PNPh · CuCl (1): space group P1, Z = 4, 3639 independent observed reflexions, R = 0.038. Lattice dimensions (18 °C): a = 1047.6; b = 1251.5; c = 1755 pm; α = 103.43°; β = 97.24°; γ = 101.30°. The compound forms monomeric molecules; the asymmetric unit contains two crystallo-graphically independent molecules. The CuCl molecule is bonded via the N atom of the phos-phoranimine. Bond lengths: Cu-N = 189 pm; Cu-CI = 209 pm; bond angle N - Cu - CI = 177°. (Ph3P)2N2C4O2(NMe) · CuCl (2): space group Pbca, Z = 8, 5611 independent, observed reflexions, R = 0.069. Lattice dimensions (25 °C): a = 1224.3; b = 1962.5: c = 2994.0 pm. The compound forms monomeric molecules with the CuCl molecule bonded via one of the N atoms of the phosphoranimine groups. Bond lengths: Cu - N = 194 pm; Cu-CI = 212 pm; bond angle N-Cu -CI -175°.

Sign in / Sign up

Export Citation Format

Share Document